CN113993284A - Preparation method of high-thermal-conductivity hole plugging resin for PCB - Google Patents
Preparation method of high-thermal-conductivity hole plugging resin for PCB Download PDFInfo
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- CN113993284A CN113993284A CN202111255574.XA CN202111255574A CN113993284A CN 113993284 A CN113993284 A CN 113993284A CN 202111255574 A CN202111255574 A CN 202111255574A CN 113993284 A CN113993284 A CN 113993284A
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/0094—Filling or covering plated through-holes or blind plated vias, e.g. for masking or for mechanical reinforcement
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Abstract
The invention discloses a preparation method of high-thermal-conductivity hole plugging resin for a PCB, which comprises the following steps: 1) adding low-dielectric-loss resin into a heat-conducting filler for preheating treatment; 2) weighing graphene, and adding a curing accelerator and an active monomer into the graphene; 3) mixing the heat-conducting filler obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer obtained in the step 2), then carrying out ball milling, adding an organic solvent, and carrying out ball milling and mixing; 4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 90-130 ℃; applying pressure for lamination; and then continuously raising the temperature and preserving the heat for a period of time to obtain the high-thermal-conductivity hole plugging resin. After the hole plugging resin prepared by the invention is cured for 20min at 140 ℃, the heat resistance temperature can reach more than 600K, the highest thermal conductivity can reach 154W/(K.m), and the linear expansion coefficient is about 17 multiplied by 10‑6And K, good temperature resistance.
Description
Technical Field
The invention belongs to the technical field of printed circuit boards, and particularly relates to a preparation method of high-thermal-conductivity hole plugging resin for a PCB.
Background
With the development of electronic information technology, electronic products are developing in the direction of light weight, miniaturization and high speed, higher requirements are put on printed boards, and the trend of smaller and denser line widths, line distances and the like is inevitably developed in the era of High Density Interconnection (HDI) technology. In order to adapt to the trend of development, printed board design and manufacturers are also continuously updating the manufacturing method of design concept and process. The technology of resin hole plugging is also a technical method invented by people in reducing the design size of the printed board and matching with the assembly of components. The design concept of the HDI packaging structure and the large-scale production of the HDI packaging structure really exert great driving force in the field of manufacturing of printed boards, and reliability and manufacturing process capability of products such as HDI, thick copper and back boards are effectively improved. Understanding and effectively utilizing this technology is also an ongoing endeavor for many print boarders. The resin hole-plugging process flow is more and more widely applied in the printed board industry in recent years, and is particularly favored on products with high layer number and large board thickness. It is desirable to use resin plugs to solve a number of problems that cannot be solved by using green oil plugs or press-fit resin plugs. However, due to the nature of the resin used in this process, the difficulty of making the resin with a high viscosity and difficult to print needs to be overcome. When some high-rise thick plates have ultramicropores (the diameter is less than 0.5 mm) and need resin hole plugging, the problems of hole plugging insufficiency, resin depression and the like are easy to occur, and the quality defect of the printed board is caused.
Disclosure of Invention
The invention mainly solves the technical problem of providing a preparation method of the high-thermal-conductivity hole plugging resin for the PCB, the prepared hole plugging resin has the heat resistance temperature of over 600K after being cured for 20min at 140 ℃, the highest thermal conductivity of 154W/(K.m) and the linear expansion coefficient of about 17 multiplied by 10-6And K, good temperature resistance.
In order to solve the technical problems, the invention adopts a technical scheme that: a preparation method of high thermal conductivity hole plugging resin for a PCB comprises the following steps:
1) adding low-dielectric-loss resin into a heat-conducting filler for preheating treatment, wherein the temperature of the preheating treatment is 150-200 ℃;
2) weighing graphene according to the mass ratio of the heat-conducting filler to the graphene of 1 (1.5-2), and adding a curing accelerator and an active monomer into the graphene;
3) mixing the heat-conducting filler obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer obtained in the step 2), performing ball milling, adding an organic solvent, and performing ball milling and mixing for 4-6 hours;
4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 90-130 ℃ at a heating rate of 2.0-3.0 ℃/min; applying a maximum pressure of 350-; and then continuously raising the temperature to control the temperature at 195-220 ℃ and preserving the heat for 110-160min to obtain the high-thermal-conductivity hole plugging resin.
In step 1), the mass ratio of the heat-conducting filler to the low-dielectric-loss resin is 1 (0.02-0.05).
In step 2), the mass of the curing accelerator is 0.02-0.05% of the mass of the graphene, and the mass of the active monomer is 0.05-0.08% of the mass of the graphene.
In step 3), the organic solvent is at least one of toluene and methyl tetrahydrofuran, and the amount of the organic solvent is 0.08-0.1% of the mass of the graphene.
Further, the particle size of the graphene is 1-5 μm.
Further, the heat conductive filler is one of boron nitride, aluminum nitride or aluminum oxide.
Further, the low dielectric loss resin is one of dicyclopentadiene epoxy resin, cyanate ester resin or benzocyclobutene resin.
Further, the active monomer is N, N-dihydroxyethyl-3-amino methyl propionate.
Further, the curing accelerator is 2-phenyl-4-methylimidazole.
The invention has the beneficial effects that:
1. the composition can simultaneously achieve heat resistance, high thermal conductivity and excellent linear expansion coefficient, can meet the technical requirements of complex electronic equipment on high-efficiency and high-cost performance thermal control in a printed circuit board, and has wide application prospect;
2. the preparation method has the advantages of simple preparation process, convenient operation and convenient source of reaction raw materials, can finish the preparation process in general equipment, and is favorable for realizing industrial production.
Detailed Description
The following detailed description of the preferred embodiments of the present invention is provided to enable those skilled in the art to more readily understand the advantages and features of the present invention, and to clearly and unequivocally define the scope of the present invention.
Example 1
A preparation method of high-thermal-conductivity hole plugging resin for a PCB comprises the following steps:
1) adding dicyclopentadiene epoxy resin into boron nitride for preheating treatment, wherein the preheating treatment temperature is 150 ℃, and the mass ratio of the boron nitride to the dicyclopentadiene epoxy resin is 1: 0.02;
2) weighing graphene with the particle size of 1 mu m according to the mass ratio of 1:1.5 of boron nitride to graphene, and adding a curing accelerator 2-phenyl-4-methylimidazole and an active monomer N, N-dihydroxyethyl-3-amino methyl propionate into the graphene, wherein the using amounts of the curing accelerator and the active monomer are 0.02% and 0.05% of the mass of the graphene respectively;
3) mixing the boron nitride obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer in the step 2), performing ball milling, adding an organic solvent toluene with the mass of 0.08% of that of the graphene, and performing ball milling and mixing at 300r/min for 4 hours to obtain a ball-milled material in a slurry shape;
4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 90 ℃ at a heating rate of 2.0 ℃/min; applying a maximum pressure of 350psi for lamination; and then continuously raising the temperature to 195 ℃, and keeping the temperature for 110min to obtain the high-thermal-conductivity hole plugging resin.
Example 2
A preparation method of high-thermal-conductivity hole plugging resin for a PCB comprises the following steps:
1) adding cyanate ester resin into aluminum nitride for preheating treatment, wherein the preheating treatment temperature is 180 ℃, and the mass ratio of the aluminum nitride to the cyanate ester resin is 1: 0.05;
2) weighing 3 mu m graphene according to the mass ratio of aluminum nitride to graphene of 1:2, and adding a curing accelerator 2-phenyl-4-methylimidazole and an active monomer N, N-dihydroxyethyl-3-amino methyl propionate into the graphene, wherein the use amounts of the curing accelerator and the active monomer are 0.05% and 0.08% of the mass of the graphene respectively;
3) mixing the aluminum nitride obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer in the step 2), performing ball milling, adding an organic solvent toluene with the mass being 0.1% of that of the graphene, and performing ball milling and mixing at 300r/min for 6 hours to obtain a ball-milled material in a slurry shape;
4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 100 ℃ at a heating rate of 2.5 ℃/min; applying a maximum pressure of 400psi for lamination; and then continuously raising the temperature to 200 ℃, and keeping the temperature for 130min to obtain the high-thermal-conductivity hole plugging resin.
Example 3
A preparation method of high-thermal-conductivity hole plugging resin for a PCB comprises the following steps:
1) adding benzocyclobutene resin into aluminum oxide for preheating treatment, wherein the preheating treatment temperature is 200 ℃, and the mass ratio of the aluminum oxide to the benzocyclobutene resin is 1: 0.04;
2) weighing graphene with the particle size of 5 microns according to the mass ratio of 1:1.7 of aluminum oxide to graphene, and adding a curing accelerator 2-phenyl-4-methylimidazole and an active monomer N, N-dihydroxyethyl-3-amino methyl propionate into the graphene, wherein the using amounts of the curing accelerator and the active monomer are 0.04% and 0.07% of the mass of the graphene respectively;
3) mixing the aluminum oxide obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer in the step 2), performing ball milling, adding an organic solvent methyl tetrahydrofuran with the mass being 0.09% of that of the graphene, and performing ball milling and mixing at 300r/min for 5 hours to obtain a ball-milled material in a slurry shape;
4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 130 ℃ at a heating rate of 3.0 ℃/min; applying a maximum pressure of 450psi for lamination; and then continuously raising the temperature to control the temperature at 220 ℃, and preserving the temperature for 160min to obtain the high-thermal-conductivity hole plugging resin.
After curing the hole plugging resins obtained in the embodiments 1, 2 and 3 at 140 ℃ for 20min, the heat resistance temperature can reach over 600K through detection; the thermal conductivity test samples prepared by the hole plugging resins of the examples 1, 2 and 3 have the thermal conductivity of 154W/(K.m) and the linear expansion coefficient of 17 multiplied by 10-6/K；
The hole plugging resin obtained in the embodiments 1, 2 and 3 is used for plugging through holes with the aperture of 200 mu m and the depth of 400 mu m on a 6-layer circuit board, and after the 288 ℃ dip soldering test for 20s, circuit board samples can resist thermal shock and circulate for 5 times without discovering the phenomenon of 'board explosion'.
Practice proves that the hole plugging resin with high thermal conductivity and good temperature resistance can be prepared by the method, and the hole plugging resin prepared by the method can be applied to the field of electronic packaging.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent structural changes made by using the contents of the present specification, or any other related technical fields directly or indirectly, are included in the scope of the present invention.
Claims (9)
1. A preparation method of high-thermal-conductivity hole plugging resin for a PCB is characterized by comprising the following steps: the method comprises the following steps:
1) adding low-dielectric-loss resin into a heat-conducting filler for preheating treatment, wherein the temperature of the preheating treatment is 150-200 ℃;
2) weighing graphene according to the mass ratio of the heat-conducting filler to the graphene of 1 (1.5-2), and adding a curing accelerator and an active monomer into the graphene;
3) mixing the heat-conducting filler obtained in the step 1) and the graphene mixed with the curing accelerator and the active monomer obtained in the step 2), performing ball milling, adding an organic solvent, and performing ball milling and mixing for 4-6 hours;
4) placing the material obtained after ball milling in the step 3) in a vacuum hot oil press, and heating to 90-130 ℃ at a heating rate of 2.0-3.0 ℃/min; applying a maximum pressure of 350-; and then continuously raising the temperature to control the temperature at 195-220 ℃ and preserving the heat for 110-160min to obtain the high-thermal-conductivity hole plugging resin.
2. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: in the step 1), the mass ratio of the heat-conducting filler to the low-dielectric-loss resin is 1 (0.02-0.05).
3. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: in the step 2), the mass of the curing accelerator is 0.02-0.05% of that of graphene, and the mass of the active monomer is 0.05-0.08% of that of graphene.
4. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: in the step 3), the organic solvent is at least one of toluene and methyl tetrahydrofuran, and the dosage of the organic solvent is 0.08-0.1% of the mass of the graphene.
5. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: the particle size of the graphene is 1-5 mu m.
6. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: the heat conducting filler is one of boron nitride, aluminum nitride or aluminum oxide.
7. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: the low dielectric loss resin is one of dicyclopentadiene epoxy resin, cyanate ester resin or benzocyclobutene resin.
8. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: the active monomer is N, N-dihydroxyethyl-3-amino methyl propionate.
9. The method for preparing the high thermal conductivity hole plugging resin for the PCB as claimed in claim 1, wherein: the curing accelerator is 2-phenyl-4-methylimidazole.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111255574.XA CN113993284A (en) | 2021-10-27 | 2021-10-27 | Preparation method of high-thermal-conductivity hole plugging resin for PCB |
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| CN202111255574.XA CN113993284A (en) | 2021-10-27 | 2021-10-27 | Preparation method of high-thermal-conductivity hole plugging resin for PCB |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115122522A (en) * | 2022-06-29 | 2022-09-30 | 南雄市科鼎化工有限公司 | Preparation method of high-thermal-conductivity resin special for PCB hole plugging |
| CN115124835A (en) * | 2022-09-01 | 2022-09-30 | 深圳市板明科技股份有限公司 | High-humidity-heat-resistant hole plugging resin and resin hole plugging method |
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| CN103881308A (en) * | 2014-04-08 | 2014-06-25 | 安捷利（番禺）电子实业有限公司 | Plugging material with high thermal conductivity and preparation method of plugging material |
| KR101573170B1 (en) * | 2015-03-23 | 2015-11-30 | 최재영 | Composite resin composition for plugging hole |
| CN105585808A (en) * | 2016-01-26 | 2016-05-18 | 广东汕头超声电子股份有限公司覆铜板厂 | Low-dielectric-loss high-heat-conductivity resin composition and preparation method thereof, and prepreg and laminated board prepared from resin composition |
| CN108521714A (en) * | 2018-04-19 | 2018-09-11 | 昆山苏杭电路板有限公司 | Wiring board jack process using grapheme material as rabbet ink |
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2021
- 2021-10-27 CN CN202111255574.XA patent/CN113993284A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881308A (en) * | 2014-04-08 | 2014-06-25 | 安捷利（番禺）电子实业有限公司 | Plugging material with high thermal conductivity and preparation method of plugging material |
| KR101573170B1 (en) * | 2015-03-23 | 2015-11-30 | 최재영 | Composite resin composition for plugging hole |
| CN105585808A (en) * | 2016-01-26 | 2016-05-18 | 广东汕头超声电子股份有限公司覆铜板厂 | Low-dielectric-loss high-heat-conductivity resin composition and preparation method thereof, and prepreg and laminated board prepared from resin composition |
| CN108521714A (en) * | 2018-04-19 | 2018-09-11 | 昆山苏杭电路板有限公司 | Wiring board jack process using grapheme material as rabbet ink |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115122522A (en) * | 2022-06-29 | 2022-09-30 | 南雄市科鼎化工有限公司 | Preparation method of high-thermal-conductivity resin special for PCB hole plugging |
| CN115122522B (en) * | 2022-06-29 | 2023-03-10 | 广东科鼎新材料股份有限公司 | Preparation method of high-thermal-conductivity resin special for PCB hole plugging |
| CN115124835A (en) * | 2022-09-01 | 2022-09-30 | 深圳市板明科技股份有限公司 | High-humidity-heat-resistant hole plugging resin and resin hole plugging method |
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Application publication date: 20220128 |